CN110270316A - Decolorising agent and preparation method thereof - Google Patents
Decolorising agent and preparation method thereof Download PDFInfo
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- CN110270316A CN110270316A CN201811513080.5A CN201811513080A CN110270316A CN 110270316 A CN110270316 A CN 110270316A CN 201811513080 A CN201811513080 A CN 201811513080A CN 110270316 A CN110270316 A CN 110270316A
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- decolorising agent
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- wool
- toluene
- catalyst
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 126
- 210000002268 wool Anatomy 0.000 claims abstract description 85
- 102000011782 Keratins Human genes 0.000 claims abstract description 57
- 108010076876 Keratins Proteins 0.000 claims abstract description 57
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 54
- 239000003054 catalyst Substances 0.000 claims abstract description 25
- 230000032050 esterification Effects 0.000 claims abstract description 23
- 238000005886 esterification reaction Methods 0.000 claims abstract description 23
- UEEJHVSXFDXPFK-UHFFFAOYSA-O N-dimethylethanolamine Chemical compound C[NH+](C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-O 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 13
- 239000011964 heteropoly acid Substances 0.000 claims abstract description 12
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000019260 propionic acid Nutrition 0.000 claims abstract description 5
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims abstract description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 24
- 239000002585 base Substances 0.000 claims description 16
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- 229960002887 deanol Drugs 0.000 claims 1
- 239000012972 dimethylethanolamine Substances 0.000 claims 1
- 239000000975 dye Substances 0.000 abstract description 45
- 239000002351 wastewater Substances 0.000 abstract description 9
- 238000005411 Van der Waals force Methods 0.000 abstract description 7
- 230000015271 coagulation Effects 0.000 abstract description 7
- 238000005345 coagulation Methods 0.000 abstract description 7
- 238000005189 flocculation Methods 0.000 abstract description 7
- 230000016615 flocculation Effects 0.000 abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 7
- 239000001257 hydrogen Substances 0.000 abstract description 7
- 150000002500 ions Chemical class 0.000 abstract description 7
- 239000000693 micelle Substances 0.000 abstract description 7
- 238000004043 dyeing Methods 0.000 abstract description 5
- 230000002209 hydrophobic effect Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 23
- 230000000694 effects Effects 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 239000000047 product Substances 0.000 description 14
- 238000001179 sorption measurement Methods 0.000 description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- 125000000129 anionic group Chemical group 0.000 description 9
- 235000011121 sodium hydroxide Nutrition 0.000 description 9
- 230000007062 hydrolysis Effects 0.000 description 8
- 238000006460 hydrolysis reaction Methods 0.000 description 8
- 102000004169 proteins and genes Human genes 0.000 description 7
- 108090000623 proteins and genes Proteins 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000005576 amination reaction Methods 0.000 description 4
- 238000004042 decolorization Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000005292 vacuum distillation Methods 0.000 description 4
- 241000883966 Astrophytum capricorne Species 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- PIEQFSVTZMAUJA-UHFFFAOYSA-N 7-hydroxy-8-{[4-(phenyldiazenyl)phenyl]diazenyl}naphthalene-1,3-disulfonic acid Chemical compound OC1=CC=C2C=C(S(O)(=O)=O)C=C(S(O)(=O)=O)C2=C1N=NC(C=C1)=CC=C1N=NC1=CC=CC=C1 PIEQFSVTZMAUJA-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 241001494479 Pecora Species 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 210000004209 hair Anatomy 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 235000014103 egg white Nutrition 0.000 description 1
- 210000000969 egg white Anatomy 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5263—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4856—Proteins, DNA
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Cosmetics (AREA)
Abstract
The present invention relates to dye fields, in particular to a kind of decolorising agent and preparation method thereof.The preparation method of decolorising agent, which specifically includes that, is blended with wool keratin, N, and the mixture of N- dimethylethanolamine, catalyst and toluene is esterified at 80 DEG C -100 DEG C, adjusts pH value to 5-6；Wherein, catalyst is one of propionic acid, the concentrated sulfuric acid and solid heteropoly acid or a variety of.It will be by N, wool keratin after the esterification of N- dimethylethanolamine is used for the decoloration of dyeing waste-water, they and dye ions and intermolecular it can produce electrostatic attraction, hydrogen bond, Van der Waals force and hydrophobic forces under suitable condition, to adsorb dyestuff or dyestuff is embedded in micelle, achieve the purpose that remove Wastewater Dyes through flocculation, coagulation.
Description
Technical field
The present invention relates to dye fields, in particular to a kind of decolorising agent and preparation method thereof.
Background technique
Someone extracts the angle in wool using sodium hydroxide and peroxide passivation using discarded wool fiber as raw material at present
Albumen.Wool protein extracting solution is used to decolourize as decolorising agent.But use wool protein extracting solution as de- in the prior art
The decolorizing effect of toner is poor.
Summary of the invention
The purpose of the present invention is to provide a kind of decolorising agent and preparation method thereof, it is intended to improve existing wool protein and mentions
The problem for taking liquid decolorizing effect poor.
First aspect present invention provides a kind of preparation method of decolorising agent, and the preparation method of decolorising agent specifically includes that
It is blended with wool keratin, N, the mixture of N- dimethylethanolamine, catalyst and toluene is at 80 DEG C -100
It is esterified at DEG C, adjusts pH value to 5-6；
Wherein, catalyst is one of propionic acid, the concentrated sulfuric acid and solid heteropoly acid or a variety of.
Inventor has found that wool keratin is poor to anionic dye decolorizing effect, be because wool keratin to it is acid,
Directly, the adsorption capacity of the anionic dyes such as activity is small.
Using the carboxyl and N of wool keratin, N- dimethylethanolamine esterification introduces in wool keratin molecule
Amido increases the cationic number in keratin after amination modifying, improves its adsorption capacity to anionic dye,
Adsorption effect is good.Will be by N, the wool keratin after the esterification of N- dimethylethanolamine is used for the decoloration of dyeing waste-water, appropriate
Under the conditions of they and dye ions and it is intermolecular can produce electrostatic attraction, hydrogen bond, Van der Waals force and hydrophobic forces, to adsorb
Dyestuff is embedded in micelle by dyestuff, achievees the purpose that remove Wastewater Dyes through flocculation, coagulation.Toluene is mainly used for dissolving
Wool keratin, N, N- dimethylethanolamine, and toluene can take away the water in solution, have and take water effect.Catalyst promotees
Into the generation of esterification.
In some embodiments of first aspect present invention, before above-mentioned adjusting pH value to 5-6 step after esterif iotacation step
It further include the toluene removed in esterification products.
Toluene in removal esterification products is conducive to purify esterification products, and the dirt of decolorization material can be treated to avoid toluene
Dye, in addition, toluene can remove together the water in esterification products while removing the toluene in esterification products.
In some embodiments of first aspect present invention, above-mentioned catalyst is solid heteropoly acid.
Solid heteropoly acid has its unique uniform acidity, and solid heteropoly acid can be improved the conversion ratio of raw material, and solid is miscellaneous
Polyacid is more advantageous to the fracture and recombination of key.
In some embodiments of first aspect present invention, before above-mentioned esterif iotacation step further include:
Wool keratin is heated to 35 DEG C -45 DEG C, then adds N, N- dimethylethanolamine, catalyst and toluene obtain
To mixture.
In some embodiments of first aspect present invention, above-mentioned wool keratin, N, N- dimethylethanolamine, catalyst
And the mass ratio of toluene is 30:10-50:0.5-2:5-10.
Be conducive to improve wool keratin, N, the utilization rate of N- dimethylethanolamine increases the conversion ratio of reactant.
In some embodiments of first aspect present invention, above-mentioned adjusting pH value to 5-6 step is specifically included: using quality
The aqueous alkali that score is 35%-45% adjusts pH value.
In some embodiments of first aspect present invention, it is above-mentioned mixing wool keratin, N, N- dimethylethanolamine,
Before catalyst and toluene step, further includes:
The mixed liquor for being blended with wool, strong base solution, hydrogen peroxide solution hydrolyzes 40-70 minutes at 80 DEG C -100 DEG C,
Removal residue obtains wool keratin.
Strong base solution, hydrogen peroxide solution mixed liquor by wool protein-COOH ,-NH2At isopolarity group
Reason, power is inhaled the effects of generation electrostatic attraction, Van der Waals force and hydrogen bond between hydrolysate wool keratin and dye ions, molecule
Dyestuff is wrapped in micelle by attached dye, through flocculation, coagulation, achievees the purpose that remove dyestuff in dyeing waste water.It simultaneously can be with
Achieve the purpose that recycle waste wool.
In some embodiments of first aspect present invention, the mass fraction of above-mentioned strong base solution is 35%-45%；Dioxygen
The mass fraction of aqueous solution is 25%-35%.
In some embodiments of first aspect present invention, above-mentioned wool, hydrogen peroxide solution, strong base solution mass ratio be
1:2.5-5:2.5-5。
Strong base solution, hydrogen peroxide solution can increase the percent hydrolysis of wool protein using aforementioned proportion, increase highly basic, double
The utilization rate of oxygen water keeps the hydrolysis of wool protein more thorough.
Second aspect of the present invention provides a kind of decolorising agent, the system of the decolorising agent decolorising agent that first aspect provides through the invention
Preparation Method is made.
Decolorising agent provided by the invention and dye ions and intermolecular it can produce electrostatic attraction, hydrogen bond, Van der Waals force and dredge
Water active force reaches the mesh for removing Wastewater Dyes through flocculation, coagulation to adsorb dyestuff or dyestuff is embedded in micelle
's.
Decolorising agent provided by the invention might as well to the decolorizing effect of the anionic dyes such as acid, direct, activity.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Decolorising agent of the embodiment of the present invention and preparation method thereof is specifically described below.
First aspect present invention provides a kind of preparation method of decolorising agent, and the preparation method of decolorising agent specifically includes that
It is blended with wool keratin, N, the mixture of N- dimethylethanolamine, catalyst and toluene is at 80 DEG C -100
It is esterified at DEG C, adjusts pH value to 5-6；
Wherein, catalyst is one of propionic acid, the concentrated sulfuric acid and solid heteropoly acid or a variety of.
In the prior art using discarded wool fiber as raw material, the keratin in wool is extracted.Inventor has found wool
Keratin is poor to anionic dye decolorizing effect, is because wool keratin is to anionic dyes such as acid, direct, activity
Adsorption capacity is small.
In the present embodiment, the carboxyl and N of wool keratin, N- dimethylethanolamine esterification, in wool keratin
Amido is introduced in molecule, and the cationic number in wool keratin is increased after amination modifying, improves it to anion
The adsorption capacity of dyestuff increases adsorption effect.Will be by N, the wool keratin after the esterification of N- dimethylethanolamine is useless for dyeing
The decoloration of water esterification products and dye ions or intermolecular can produce electrostatic attraction, hydrogen bond, Van der Waals force under suitable condition
And hydrophobic forces reach through flocculation, coagulation to adsorb dyestuff or dyestuff is embedded in micelle and remove Wastewater Dyes
Purpose.
Following reaction occurs for wool keratin, N, N- dimethylethanolamine:
- COOH+HOCH2CH2N(CH3)2→-COOCH2CH2N(CH3)2
Toluene is mainly used for dissolving wool keratin, N, N- dimethylethanolamine, and toluene can be by the water band in solution
It walks, has and take water effect.The generation of catalyst promotion esterification.
Further, solid heteropoly acid has its unique uniform acidity, and solid heteropoly acid can be improved the conversion of raw material
Rate, solid heteropoly acid are more advantageous to the fracture and recombination of key.
It further, further include the toluene removed in esterification products after esterif iotacation step before adjusting pH value to 5-6 step.
Toluene in removal esterification products is conducive to purify esterification products, and the dirt of decolorization material can be treated to avoid toluene
Dye, in addition, toluene can take away the water in esterification products while removing the toluene in esterification products.
In some embodiments of first aspect present invention, above-mentioned wool keratin, N, N- dimethylethanolamine, catalyst
And the mass ratio of toluene is 30:10-50:0.5-2:5-10.
Wool keratin, N, the mass ratio of N- dimethylethanolamine, catalyst and toluene is in 30:10-50:0.5-2:5-
In 10 ranges, further, wool keratin, N, the mass ratio of N- dimethylethanolamine, catalyst and toluene are 30:20-
30:1-1.5:6-8。
Be conducive to improve wool keratin, N, the utilization rate of N- dimethylethanolamine increases the conversion ratio of reactant.
It should be noted that in other embodiments of the invention, can according to physical condition, without consider reactant,
The product of catalyst and toluene and use other raw material proportionings.
Further, it adjusts pH value to 5-6 step to specifically include: the aqueous alkali tune for using mass fraction as 35%-45%
Save pH value.
In the present embodiment, pH value is adjusted using the sodium hydroxide of 35%-45% or potassium hydroxide；It is understood that
It is that in other embodiments of the invention, pH value, such as ammonium hydroxide can be adjusted using other substances.
In the present embodiment, mixture is made by following steps:
Wool keratin is heated to 35 DEG C -45 DEG C, then adds N, N- dimethylethanolamine, catalyst and toluene obtain
To mixture.
Wool keratin is first heated to 35 DEG C -45 DEG C, improves the dissolubility of wool keratin, makes wool keratin molecule
It more fully spreads, further with N, the reaction of N- dimethylethanolamine is sufficiently；Make carboxyls more as far as possible by amination, improves it to yin
The adsorption capacity of ionic dye increases adsorption effect.
Further, in the present embodiment, wool keratin is as made from wool.
In detail, wool, strong base solution, hydrogen peroxide solution are mixed to get mixed liquor, by mixed liquor at 80 DEG C -100 DEG C
Lower hydrolysis 40-70 minutes, removal residue obtain wool keratin.
Wool can be new wool or discarded wool.
Discarded wool is a kind of source biomass extremely abundant, and a kind of important, cheap keratin resource it
One, it is worth with high research and utilization.
The mixed liquor for being blended with wool, strong base solution, hydrogen peroxide solution hydrolyzes 40-70 minutes at 80 DEG C -100 DEG C,
Removal residue obtains wool keratin.
Strong base solution, hydrogen peroxide solution by wool protein-COOH ,-NH2The processing of isopolarity group, hydrolysis produce
Electrostatic attraction, Van der Waals force are generated between object wool keratin and dye ions, molecule and the effects of hydrogen bond power absorption dyestuff or
Dyestuff is wrapped in micelle, through flocculation, coagulation, achievees the purpose that remove dyestuff in dyeing waste water.
In addition, in the present embodiment, obtaining wool keratin solution after wool hydrolysis removal residue can be esterified.
There is a part of water after wool hydrolysis, toluene can remove the water generated after esterification.
Again to the adsorption capacity that can be greatly increased after wool keratin amination modifying to anionic dye.
Further, the mass fraction of above-mentioned strong base solution is 35%-45%；The mass fraction of hydrogen peroxide solution is
25%-35%.Keep the hydrolysis of wool protein more thorough.Further, the mass fraction of strong base solution is 40%；Dioxygen is water-soluble
The mass fraction of liquid is 30%.
The mass ratio of wool and strong base solution is 1:2.5-5:2.5-5.
Increase the percent hydrolysis of wool protein, increase the utilization rate of highly basic, hydrogen peroxide, avoids in hydrating solution containing excessive
Alkali and hydrogen peroxide.It is understood that in other embodiments of the invention, the quality of strong base solution, hydrogen peroxide solution
Score may be other values, and correspondingly, ratio may be other values.
In the present embodiment, above-mentioned strong base solution can be sodium hydroxide solution, potassium hydroxide solution etc..
In the present embodiment, above-mentioned esterification carries out in a water bath.
Second aspect of the present invention provides a kind of decolorising agent, and decolorising agent is made by the preparation method of above-mentioned decolorising agent.
Decolorising agent provided by the invention and dye ions and intermolecular it can produce electrostatic attraction, hydrogen bond, Van der Waals force and dredge
Water active force reaches the mesh for removing Wastewater Dyes through flocculation, coagulation to adsorb dyestuff or dyestuff is embedded in micelle
's.
Decolorising agent provided by the invention is not only to the good decolorizing effect of anionic dye, to acid, direct, activity etc.
The decolorizing effect of anionic dye might as well.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of decolorising agent is present embodiments provided, which is mainly made by following steps:
Prepare goat's horn albumen: sodium hydrate aqueous solution, the 250g 35wt% of wool, 250g 35wt% that 100g is cleaned
Hydrogen peroxide mixing, in 80 DEG C of water-bath shake 60min be hydrolyzed, hydrolyzate is then filtered to remove undissolved wool
Residue obtains keratin solution.
Prepare decolorising agent: four mouthfuls for taking the above-mentioned wool keratin investment of 300g with agitating device, water segregator and condenser
In flask, 100gN is added after being heated to 40 DEG C, N- dimethylethanolamine, 0.50g propionic acid and 50g toluene are passed through recirculation water, rise
Temperature reacts 4h to 80 DEG C at reflux, and after reaction, vacuum distillation removes toluene.Solution is adjusted with 45wt%KOH
PH value is 5, obtains decolorising agent.
Embodiment 2
A kind of decolorising agent is present embodiments provided, which is mainly made by following steps:
Prepare goat's horn albumen: sodium hydrate aqueous solution, the 500g 25wt% of wool, 500g 45wt% that 100g is cleaned
Hydrogen peroxide mixing, in 100 DEG C of water-bath shake 60min be hydrolyzed, hydrolyzate is then filtered to remove undissolved sheep
Hair residue, obtains keratin solution.
Prepare decolorising agent: four mouthfuls for taking the above-mentioned wool keratin investment of 300g with agitating device, water segregator and condenser
In flask, the N of 500g is added after being heated to 40 DEG C, N- dimethylethanolamine, the 20g concentrated sulfuric acid and 100g toluene are passed through recirculation water,
90 DEG C of heating, reacts 4h at reflux, and after reaction, vacuum distillation removes toluene.Solution is adjusted with 35wt%NaOH
PH value be 6, obtain decolorising agent.
Embodiment 3
A kind of decolorising agent is present embodiments provided, which is mainly made by following steps:
Prepare goat's horn albumen: sodium hydrate aqueous solution, the 400g 30wt% of wool, 200g 40wt% that 100g is cleaned
Hydrogen peroxide mixing, in 100 DEG C of water-bath shake 60min be hydrolyzed, hydrolyzate is then filtered to remove undissolved sheep
Hair residue, obtains keratin solution.
Prepare decolorising agent: four mouthfuls for taking the above-mentioned wool keratin investment of 300g with agitating device, water segregator and condenser
In flask, the N of 400g is added after being heated to 40 DEG C, N- dimethylethanolamine, the 10g concentrated sulfuric acid and 100g toluene are passed through recirculation water,
90 DEG C of heating, reacts 4h at reflux, and after reaction, vacuum distillation removes toluene.Solution is adjusted with 35wt%NaOH
PH value be 6, obtain decolorising agent.
Embodiment 4
A kind of decolorising agent is present embodiments provided, which is mainly made by following steps:
It takes 300g wool keratin investment in the four-hole boiling flask of agitating device, water segregator and condenser, is heated to 40
The N of 300g is added after DEG C, N- dimethylethanolamine, 10g solid heteropoly acid and 80g toluene are passed through recirculation water, it heats up 95 DEG C,
4h is reacted under reflux state, after reaction, vacuum distillation removes toluene.It is 5.5 with the pH value that 40wt%KOH adjusts solution,
Obtain decolorising agent.
Embodiment 5
A kind of decolorising agent is present embodiments provided, which is mainly made by following steps:
Take 300g wool keratin, 200gN, N- dimethylethanolamine, 1.50g catalyst and the mixing of 60g toluene, 80
It is esterified at DEG C, adjusts pH value to 5.5, obtain decolorising agent.
Embodiment 6
A kind of decolorising agent is present embodiments provided, which is mainly made by following steps:
300g wool keratin, 250gN are taken, N- dimethylethanolamine, 1.20g catalyst and 70g toluene mix,
It is esterified at 100 DEG C, the toluene removed in esterification products adjusts pH value to 6 again, obtains decolorising agent.
Comparative example
The sodium hydrate aqueous solution of wool, 250g 35wt% that 100g is cleaned, the hydrogen peroxide of 250g 35wt% mix,
60min is shaken in 80 DEG C of water-bath to be hydrolyzed, and hydrolyzate is then filtered to remove undissolved wool residue, obtains angle egg
White solution.
This comparative example is used using above-mentioned keratin solution as decolorising agent.
Experimental example
The decolorising agent of decolorising agent, comparative example offer that Example 1- embodiment 6 provides is respectively to Acid Brilliant Scarlet GR
(Brilliant Crocein), direct yellow R, Reactive Brilliant Blue KN-R fabric carry out decolorization experiment under the same conditions, experiment knot
Fruit is as shown in table 1.
The bleaching agent bleaching effect of each embodiment of table 1 and comparative example compares
It can be seen from Table 1 that decolorising agent, that is, wool keratin that comparative example provides is very limited to the adsorption rate of dyestuff, it is real
Obviously increasing to the adsorption effect of dyestuff for the offer of 1- embodiment 6 is applied, percent of decolourization is all larger than 90%.
Illustrate the good decolorizing effect of decolorising agent provided in an embodiment of the present invention, method provided in an embodiment of the present invention is to wool
The decolorizing effect of keratin has the promotion of matter.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of decolorising agent, which is characterized in that the preparation method of the decolorising agent specifically includes that
It is blended with wool keratin, N, the mixture of N- dimethylethanolamine, catalyst and toluene is at 80 DEG C -100 DEG C
Esterification adjusts pH value to 5-6；
Wherein, the catalyst is one of propionic acid, the concentrated sulfuric acid and solid heteropoly acid or a variety of.
2. the preparation method of decolorising agent according to claim 1, which is characterized in that the adjusting pH value to 5-6 step it
It further include the toluene removed in esterification products after the preceding esterif iotacation step.
3. the preparation method of decolorising agent according to claim 1, which is characterized in that the catalyst is solid heteropoly acid.
4. the preparation method of decolorising agent according to claim 1, which is characterized in that before the esterif iotacation step further include:
The wool keratin is heated to 35 DEG C -45 DEG C, then adds the N, N- dimethylethanolamine, the catalyst with
And the toluene obtains the mixture.
5. the preparation method of decolorising agent according to claim 1, which is characterized in that the wool keratin, the N, N-
The mass ratio of dimethylethanolamine, the catalyst and the toluene is 30:10-50:0.5-2:5-10.
6. the preparation method of decolorising agent according to claim 1, which is characterized in that the adjusting pH value to 5-6 step has
Body includes: that mass fraction is used to adjust pH value for the aqueous alkali of 35%-45%.
7. the preparation method of decolorising agent according to claim 1-6, which is characterized in that mixing the wool angle
Albumen, the N, before N- dimethylethanolamine, the catalyst and the toluene step, further includes:
The mixed liquor for being blended with wool, strong base solution, hydrogen peroxide solution hydrolyzes 40-70 minutes at 80 DEG C -100 DEG C, removal
Residue obtains the wool keratin.
8. the preparation method of decolorising agent according to claim 7, which is characterized in that the mass fraction of the strong base solution is
35%-45%；The mass fraction of the hydrogen peroxide solution is 25%-35%.
9. the preparation method of decolorising agent according to claim 7, which is characterized in that the wool, the hydrogen peroxide solution,
The mass ratio of the strong base solution is 1:2.5-5:2.5-5.
10. a kind of decolorising agent, which is characterized in that the decolorising agent passes through the system of the described in any item decolorising agents of claim 1-9
Preparation Method is made.
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